A sensitive and selective solid phase extraction procedure for the determination of traces of Cd(II), Zn(II) and Ag(I) ions has been developed. An alumina-sodium dodecyl sulfate (SDS) coated on with 2,3 Di Hydro 2,3 paratolyl Qinazoline (1 H)- 4 one (DPTQO). The influences of the analytical parameters including pH and sample volume were investigated. Common coexisting ions did not interfere on the separation and determination of analytes under study. The adsorbed analytes were desorbed by using 6mL of 4 mol L−1 nitric acid. The responses are linear 0.02– 0.85 μg mL-1 for Cd2+ ion0.01–0.90 μg mL-1 for Zn2+and0.02–0.92μg mL-1for Ag+ detection limit for Cd(II), Zn(II) and Ag(I) ions were found to be 1.4, 1.3 and1.12(ng mL-1), respectively. It was found that the recovery for Cd2+, Zn2+and Ag+ ions were 97.7, 98.2 and 98.0 with RSD of 1.9, 1.8 and 1.7. It was also observed that recovery for repeated recovery on the same solid phase not varies more than 3%. The presented procedure was successfully applied for determination of analytes in radiology wastewater, amalgam, natural water and blood samples.